Kits were developed for labeling sulphur microcolloids with99mTc. The microcolloids were prepared to get the desired particle size. The stannous chloride was treated with sulphide ions released from thioacetamide in the presence of carboxymethyl cellulose and the pH of the reaction was adjusted to 3.0. The contents of single reaction vial were reacted with99mTc, the radiochemical yield was higher than 95%. Sulphur-microcolloid kits were stable and the stability was followed for 6 hours. The freeze-dried kits were followed more than three months after production and were found stable. Bone marrow uptake in rabbits was determined to be about 36%. The preparation of99mTc-sulphur microcolloid is performed in single step process and axellent node scintigraphy was obtained using experimental animal.